反应详情

Sodium hydride (60% dispersion in oil) (83 mg, 3.46 mmol) was added to tert-butyl 3-hydroxyazetidine-1-carboxylate (J Med chem., 44(1), 2001, 94) (0.3 g, 1.73 mmol) in THF (10 mL), at 0° C., under argon. The reaction was stirred for 30 mins then iodomethane (0.13 mL, 4.15 mmol) added. After stirring at 0° C. for 30 mins and at RT for 3 hours the volatiles were removed in vacuo. Ethyl acetate (40 mL) was added and the mixture washed with brine (40 mL), dried (MgSO4), filtered, and reduced in vacuo to give the desired compound. (0.32 g). 1H NMR δ (CDCl3): 1.42 (s, 9H), 3.27 (s, 3H), 3.81 (m, 2H), 4.06 (m, 2H), 4.11 (m, 1H).

1. stirringAfter stirring at 0° C. for 30 mins and at RT for 3 hours the volatiles
2. customwere removed in vacuo
3. additionEthyl acetate (40 mL) was added
4. washthe mixture washed with brine (40 mL)
5. dry with materialdried (MgSO4)
6. filtrationfiltered